Allyl alcohol methyl terminated polyether as well as preparation method and application thereof

A technology of allyl alcohol methyl capping and allyl alcohol polyether, which is applied in the directions of ether preparation, botanical equipment and method, application, etc., and can solve the problem of wide molecular weight distribution and primary hydroxyl content of allyl alcohol methyl capped polyether. It can achieve the effect of high double bond retention rate, narrow molecular weight distribution and high reactivity

Pending Publication Date: 2019-10-08
JIANGSU CHANGHUA POLYURETHANE SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the technical problems to be solved by the present invention is the problem of wide molecular weight distribution, low primary hydroxyl content and narrow application range of allyl alcohol methyl-terminated polyether in the prior art, and a new allyl alcohol methyl-terminated polyether is provided. polyether

Method used

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  • Allyl alcohol methyl terminated polyether as well as preparation method and application thereof
  • Allyl alcohol methyl terminated polyether as well as preparation method and application thereof
  • Allyl alcohol methyl terminated polyether as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1, add allyl alcohol 100g in 5L autoclave, adopt the phosphazene catalyst of general formula (IV) in the present invention (wherein R is methyl, R 1 is methyl) 0.82g, feed 207g of propylene oxide, the reaction temperature is 75~85 ℃, nitrogen is replaced 3 times, after adding, ripening until the pressure does not drop, to obtain allyl alcohol polyether material I, the allyl alcohol The polyether material I is shown in step 1 of Table 1;

[0036] 2. Feed 727 g of ethylene oxide, and react material I with ethylene oxide again. The reaction temperature is 90 to 100 ° C, and nitrogen is replaced for 3 times. After adding, it is aged until the pressure does not drop to obtain allyl alcohol polyether material II. , the allyl alcohol polyether material II is shown in step 2 of table 1.

[0037] 3. The allyl alcohol polyether material II of step 2 was put into 102.3 g of solid sodium methoxide, replaced with nitrogen for 3 times, and the stirring was started. Remove methanol ...

Embodiment 2 to 8 and comparative example 1 to 3

[0040] The experiments of Examples 2 to 8 and Comparative Examples 1 to 3 were carried out according to the steps of Example 1, and the only difference was that the types of reaction raw materials, catalyst types, raw material ratios, reaction times and temperatures were different. See Table 1 for details. The product quality of the obtained allyl alcohol methyl-terminated polyether is shown in Table 3.

[0041] The raw material weight percentage of each component in Table 1 Example 1 to Example 5

[0042]

[0043]

[0044] The raw material weight percentage of each component in Table 2 Examples 6 to 8 and Comparative Examples 1 to 3

[0045]

[0046]

[0047]

[0048] Table 3 Quality inspection data of allyl alcohol methyl-terminated polyethers prepared in Examples 1 to 8 and Comparative Examples 1 to 3

[0049] molecular weight Capping rate (%) Double bond retention rate (%) Molecular weight distribution coefficient Example 1 600 98 9...

Embodiment 9

[0056] The allyl alcohol block methyl-terminated refined ether prepared in Example 1 was used to prepare the polyurethane foam stabilizer with the formula, reaction temperature and reaction time shown in Table 4.

[0057] Table 4 prepares the formula of polyurethane foam stabilizer (unit: kg)

[0058]

[0059] The polyurethane foam stabilizer prepared in Example 9 was foamed with the formula of the typical free-rising polyurethane foam shown in Table 5 to prepare a polyurethane foam, and the obtained polyurethane foam was soft to the touch, and the openings were fine and uniform.

[0060] Table 5 Typical formulations of free-rising polyurethane foams

[0061] Unit: parts by weight

[0062] raw material Recipe 1 Polyether polyol (CHE-2045) 99 Polyurethane foam stabilizer in embodiment 9 1 h 2 o

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Abstract

The invention relates to an allyl alcohol methyl terminated polyether as well as a preparation method and application thereof, and mainly solve the problem that an allyl alcohol methyl terminated polyether formed by grafting propylene oxide and ethylene oxide onto allyl alcohol and performing end capping by using methyl has wide molecular weight distribution, a low primary hydroxyl content, and anarrow application range in the prior art. The method provided by the invention adopts the technical solution of preparing the allyl alcohol methyl terminated polyether with a molecular weight distribution coefficient of 1.03 to 1.21 by adopting a synthetic method of the allyl alcohol methyl terminated polyether and a phosphazene catalyst to better solve the problem, and can be used in productionof the allyl alcohol methyl terminated polyether.

Description

technical field [0001] The invention relates to a preparation method and application of an allyl alcohol methyl-terminated polyether, in particular to a preparation method and application of synthesizing allyl alcohol methyl-terminated polyether by using a phosphazene catalyst. Background technique [0002] In the prior art, the allyl alcohol polyether synthesized by the alkali catalyst of KOH, NaOH or sodium methoxide has the disadvantages of small relative molecular weight and wide molecular weight distribution. Using bimetallic DMC as a catalyst for the reaction, the reaction has an induction period and a high reaction temperature. It cannot be directly capped with ethylene oxide to obtain primary hydroxyl groups. The head-to-tail (H-T) selectivity of polyether molecules is low, and the products have ultra-high molecular weight. Smearing phenomenon, high starting agent requirements. In addition, both of the above two catalysts contain metal components, which remain in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/331C08G65/337C09D7/47C08J9/00C08L75/04C08L71/02C07C43/15A01N25/30A01N25/04C07C41/16
CPCA01N25/04A01N25/30C07C43/15C08G65/2609C08G65/2675C08G65/331C08G65/337C08J9/0061C08J2375/04C08J2471/02C09D7/47
Inventor 茅金龙高晨栋张浩陈凤秋
Owner JIANGSU CHANGHUA POLYURETHANE SCI & TECH
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